Phosphorus-nitrogen flame retardant and preparation method thereof

A flame retardant, phosphorus and nitrogen technology, applied in the field of flame retardant, can solve problems such as hazards, threats to life and property safety, etc., and achieve the effect of high yield and mild reaction conditions

Inactive Publication Date: 2014-04-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Polymers are widely used in industrial production and people's daily life, but most polymers are flammable. Most of them will be ignited and burned when encountering a fire source in the air. The molten droplets produced by combustion can also ignite

Method used

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  • Phosphorus-nitrogen flame retardant and preparation method thereof
  • Phosphorus-nitrogen flame retardant and preparation method thereof
  • Phosphorus-nitrogen flame retardant and preparation method thereof

Examples

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preparation example Construction

[0016] The preparation method of the phosphorus-nitrogen type flame retardant of the present invention is: using organic amine, hypophosphorous acid and fatty aldehyde as raw materials to react and synthesize the phosphorus-nitrogen type flame retardant containing two elements of phosphorus and nitrogen under acid catalysis; wherein, the organic amine is the molecular formula NH 2 RNH 2 One or more than one dibasic primary amines, R can be -(CH 2 ) m -, -[CH 2 CH 2 NH] p CH 2 CH 2 -or-C 6 h 4 -, m and p are all positive integers and 6≥m≥2, 4≥p≥1; fatty aldehyde is one or more of formaldehyde, acetaldehyde, propionaldehyde or butyraldehyde.

[0017] The organic amine of the present invention can be that molecular formula is NH 2 RNH 2 A dibasic primary amine, which can also be a molecular formula of NH 2 RNH 2 A mixed dibasic primary amine of two or more dibasic primary amines. NH 2 RNH 2 It may be ethylenediamine, propylenediamine, butylenediamine, pentamethyle...

Embodiment 1

[0023] Example 1 Add the raw material ethylenediamine, hypophosphorous acid and formaldehyde solution (30% concentration) with a molar ratio of ethylenediamine, hypophosphorous acid and formaldehyde of 1:3:3 into the reaction kettle, and add hydrochloric acid solution (the hydrochloric acid in the system provides H + The concentration is 0.004mol / L), after stirring evenly, the temperature rises to 75°C and reacts for 4 hours. After the reaction is completed, it is filtered, and the filter cake is washed with acetone, dichloromethane and deionized water successively, and dried in vacuum to obtain a dark yellow solid, namely It is the phosphorus nitrogen type flame retardant of the present invention. When it is used in flame-retardant epoxy resin, the phosphorus-nitrogen type flame retardant synthesized here alone can make the horizontal combustion level reach FH-1 level when the dosage is 18%.

Embodiment 2

[0024] Example 2 Add diethylenetriamine, hypophosphorous acid and formaldehyde solution (30% concentration) of diethylenetriamine, hypophosphorous acid and formaldehyde in a molar ratio of 1:3:4 to the reaction kettle, and add hydrochloric acid-sulfuric acid mixed solution (the 36% concentrated hydrochloric acid of hydrochloric acid-sulfuric acid mixed solution: 98% concentrated sulfuric acid is 5: 1 (mass ratio), the H that hydrochloric acid-sulfuric acid mixed solution provides in the system + The concentration is 0.006mol / L), after stirring evenly, the temperature rises to 85°C and reacts for 3 hours. After the reaction is completed, it is filtered, and the filter cake is washed with acetone, dichloromethane and deionized water successively, and dried in vacuum to obtain a dark yellow solid, namely It is the phosphorus nitrogen type flame retardant of the present invention. It is used for flame-retardant epoxy resin, and when the phosphorus-nitrogen type flame retardant syn...

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Abstract

The invention provides a phosphorus-nitrogen flame retardant and a preparation method thereof. The phosphorus-nitrogen flame retardant is synthesized through condensation and addition and electrophilic addition reaction of the raw materials including organic amines, hypophosphorous acid and fatty aldehydes in the presence of acid catalysts, wherein the organic amines are one or more than one of primary diamines with molecular formula of NH2RNH2, wherein R is -(CH2)m<->, -[CH2CH2NH]pCH2CH2<-> or -C6H4<->, m and p are positive integers, m is not more than 6 and not less than 2, and p is not more than 4 and not less than 1; fatty aldehydes are one or more than one of formaldehyde, acetaldehyde, propionaldehyde or butyraldehyde; the adopted acid catalysts can be one or more than one of hydrochloric acid, sulfuric acid or nitric acid. The mole ratio of the organic amines to hypophosphorous acid to fatty aldehydes adopted in the preparation process is preferably 1:(2-5):(2-5), the reaction temperature is preferably 70-90 DEG C, and the reaction time is preferably 2-6 hours.

Description

1. Technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a phosphorus-nitrogen type flame retardant and a preparation method thereof, and belongs to the field of flame retardancy. 2. Background technology [0002] Polymers are widely used in industrial production and people's daily life, but most polymers are flammable. Most of them will be ignited and burned when encountering a fire source in the air. The molten droplets produced by combustion can also ignite other combustibles. It poses a huge threat and harm to people's life and property safety, so the flame retardant problem of polymers has been widely concerned, and the research and development of flame retardants for polymers has become a hot spot. [0003] With the promulgation of environmental protection policies in various countries around the world, the green and environmental protection of flame retardants is the current development trend of flame reta...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C08G79/04C07F9/30C08L63/00C08L85/02
Inventor 应宗荣吴树文何谦张元中
Owner NANJING UNIV OF SCI & TECH
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